CN106268614A - A kind of preparation method of magnesium hydroxyapatite adsorbent - Google Patents
A kind of preparation method of magnesium hydroxyapatite adsorbent Download PDFInfo
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- CN106268614A CN106268614A CN201610905507.0A CN201610905507A CN106268614A CN 106268614 A CN106268614 A CN 106268614A CN 201610905507 A CN201610905507 A CN 201610905507A CN 106268614 A CN106268614 A CN 106268614A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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Abstract
The invention discloses the preparation method of a kind of magnesium hydroxyapatite adsorbent, it is characterized in that, with calcium nitrate, magnesium nitrate and ammonium phosphate salt as raw material, precursor solution is configured for solvent with distilled water, precursor solution is uniformly mixed to form white precipitate through chemical precipitation technique, through repeatedly centrifuge washing, 80 DEG C dried 600 800 DEG C are thermally treated resulting in magnesium hydroxyapatite adsorbent.The present invention is with chemical precipitation method simple to operate, and inexpensive calcium nitrate, magnesium nitrate and ammonium phosphate salt are precursor, has prepared heavy metals ionic adsorption magnesium hydroxyapatite adsorbent, and compared with other preparation method, present invention process is simple, with low cost.
Description
Technical field
The invention belongs to heavy metal-polluted water-treatment technology field, the preparation of a kind of magnesium-hydroxyapatite adsorbent
Method.
Background technology
In recent years, along with China's mining, ore dressing, smelt, electroplate, chemical industry, the fast development of the industry such as process hides and papermaking, produce
Give birth to the industrial wastewater of the heavy metal ion such as substantial amounts of leaded, hydrargyrum, chromium, cadmium, nickel, copper, zinc.These heavy metal wastewater therebies unreasonable
Discharge causes the heavy metal pollution of water environment, soil environment, and therefore serious threat human health.The most effectively administer
Heavy metal environmental pollution has become one of focus of world today's concern.
The method of heavy metal ion in water that removes has a lot, and traditional method has chemical reaction precipitation, physical absorption, ion
Exchange, organic group complexation and sequestration, bioanalysis, catalysis reduction etc., wherein absorption method is the sewage of a kind of great application potential
Purification techniques, uses Heavymetal Wastewater Treatment by Adsorption, it may be achieved pollution control and the unification of changing waste into resources, meets circulation warp
Ji and the requirement of sustainable development.And in actual sewage processing procedure, the selection of adsorbent key often.Therefore, find
Efficient adsorbent becomes the focus of current research for sewage purification.
Hydroxyapatite [Ca10(PO4)6(OH)2] be two kinds there is good physicochemical property and biology performance, simultaneously its point
Son is owing to having excellent gap structure and chemism hydroxyl and Ca2+Structure is widely used in heavy metal in aqueous systems
Adsorption treatment, simultaneously as have good harmony with environment, does not easily cause secondary pollution, thus becomes a kind of novel environmental merit
Energy material, by people's strong interest.But hydroxyapatite itself is due to hexagonal crystallographic texture, causes being difficult to of crystals
Replaced by metal ion and and metal ion exchanged, cause absorption property limited, it is thus desirable to hydroxyapatite is changed
Property, improve adsorbable group number in its specific surface area and molecule and and heavy metal between exchange degree.
Some scholars attempt mixing carbonate in hydroxyapatite lattice, make the structure of hydroxyapatite be distorted,
Degree of crystallinity declines, and specific surface area increases, and is more beneficial for the absorption of heavy metal ion.Such as patent: a kind of carbonate hydroxyapatite
The preparation method (ZL201210298413.3) of superfine nanowire;Patent: a kind of carbon light base apatite with reproducibility function
Synthetic method (CN2015100460298);Patent: a kind of high-carbon acid group doping carbon through base apatite adsorbent preparation and
Application (CN201610110910.4)).But the major way of these doping carbonates is to use the inorganic chemical containing carbonate
Thing carries out high-temperature calcination sintering, therefore, it is difficult to the doping ratio of carbonate during ensureing doping, carbonate is difficult to adulterate simultaneously
Inside hydroxyapatite, causing carbonate doping ratio low, specific surface area is low, and absorption property is limited.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, a kind of magnesium-hydroxyl in heavy metal-polluted water technology is provided
The preparation method of base apatite adsorbent, uses the magnesium ion (radius: 72pm) less than calcium ion (radius: 100pm) to hydroxyl
Apatite is doped, it is easier to make the structure of hydroxyapatite be distorted, and degree of crystallinity declines, and specific surface area increases, permissible
Accelerate during Adsorption of Heavy Metal Ions and increase ion exchange.Solve hydroxyapatite as sewage at
The adsorbent of reason, specific surface area its adsorption capacity little is low, conventional carbonate doped hydroxyapatite external carbon acid group source, and
The problems such as poor selectivity.
In order to achieve the above object, the present invention uses following technical proposal:
A kind of preparation method of magnesium-hydroxyapatite adsorbent, with calcium nitrate, magnesium nitrate and ammonium phosphate salt as raw material, with
Distilled water is that solvent configures precursor solution, and through chemical precipitation technique, precursor solution is uniformly mixed to form white precipitate, warp
Crossing repeatedly centrifuge washing, 80 DEG C dried 600-800 DEG C is thermally treated resulting in magnesium-hydroxyapatite adsorbent.
Further, the preparation of described precursor solution: the calcium nitrate (Ca (NO of the 0.1-1mol/L being respectively configured3)2) water-soluble
Liquid, the magnesium nitrate (Mg (NO of 0.1-1mol/L3)2) aqueous solution, the saline solution of ammonium phosphate of 0.06-0.6mol/L, each stirring is all
Even obtain three kinds of precursor solution.
Further, described chemical precipitation technique: under normal temperature condition, by the molfraction of magnesium ion/(calcium ion+magnesium ion)
For 5-15%, calcium nitrate and magnesium nitrate precursor solution are mixed, then this mixed solution is added drop-wise to body before ammonium phosphate salt
In liquid solution, wherein the mol ratio of (calcium+magnesium)/phosphorus is 1.67, is stirred continuously simultaneously, and in reaction, constantly dropping ammonia makes mixing molten
The pH value of liquid is constant at 10-12;After precursor solution drips, continue stirring 1-2h, to ensure fully reaction, obtain white
Mixed solution;Then being aged 8-24 hour by mixed solution, mixture is divided into two-layer, and upper strata is settled solution, and lower floor is white
Precipitation.(defining that hybrid mode has certain step here, not three are mixed together.Before being because calcium nitrate and magnesium nitrate
Body solution provides the cation of reaction, and both solution will not react, and they first be mixed, it is ensured that below
The uniformity of reaction.Additionally, pH value is the essential condition obtaining product, the lowest impurity that may produce other is the highest
Can't obtain more preferable result, waste ammonia on the contrary.)
Further, described centrifuge washing technique: mixture is centrifuged, and carry out with the distilled water precipitate to obtaining
Cleaning, repeated centrifugation is cleaned 2-3 time, then uses ethanol purge 1-2 time;The terpineol ethanol solution of configuration 5%, and press solid-liquid
In the white depositions finally obtained, add appropriate terpineol ethanol solution than about 1g/ml, stir.
Further, described Technology for Heating Processing: the white mixture obtained is put into baking oven, dry 12-24h, obtain for 80 DEG C
White powder, then at 600-800 DEG C of calcining, is incubated 2-4h, obtains heavy metals ionic adsorption magnesium-hydroxylapatite adsorption
Agent.
Above-mentioned ammonium phosphate salt is ammonium phosphate, ammonium hydrogen phosphate, one or more mixture of ammonium dihydrogen phosphate.
The invention has the beneficial effects as follows:
(1) present invention is front body with chemical precipitation method simple to operate, inexpensive calcium nitrate, magnesium nitrate and ammonium phosphate salt
Body, has prepared heavy metals ionic adsorption magnesium-hydroxyapatite adsorbent, compared with other preparation method, work of the present invention
Skill is simple, with low cost.
(2) method of the present invention uses the magnesium ion (radius: 72pm) less than calcium ion (radius: 100pm) to hydroxyl
Base apatite is doped, it is easier to make the structure of hydroxyapatite be distorted, and degree of crystallinity declines, and specific surface area increases, can
To accelerate during Adsorption of Heavy Metal Ions and to increase ion exchange.
(3) method of the present invention uses the ethanol solution dispersant as white precipitate of terpineol, effectively
The white predecessor prevented reunion in heat treatment process, the magnesium-hydroxyapatite adsorbent obtained is evenly distributed, granule chi
Very little reach Nano grade.Through experiment, compared with simple hydroxyapatite adsorbent, this ABSORBENTS ABSORPTION adsorption of metal ions
Ability is greatly improved.
Accompanying drawing explanation
Fig. 1 is magnesium-hydroxyapatite adsorbent XRD figure spectrum that the present invention obtains;
Fig. 2 is magnesium-hydroxyapatite adsorbent transmission electron microscope photo that the present invention obtains;
Fig. 3 is to invent the magnesium-hydroxyapatite adsorbent obtained to the adsorption curve of copper ion in copper sulfate solution.
Detailed description of the invention
Heavy metals ionic adsorption magnesium-hydroxy-apatite of the present invention is further described below by way of specific embodiment
The preparation process of stone adsorbent, but it is not limited to this.
Embodiment 1
1, the preparation of precursor solution: the calcium nitrate (Ca (NO of the 0.1mol/L being respectively configured3)2) aqueous solution, 0.1mol/L
Magnesium nitrate (Mg (NO3)2) aqueous solution, the ammonium hydrogen phosphate ((NH of 0.06mol/L4)2HPO4) aqueous solution, each it is uniformly mixing to obtain
Three kinds of precursor solution;
2, chemical precipitation technique: under normal temperature condition, is 15% general by the molfraction of magnesium ion/(calcium ion+magnesium ion)
Calcium nitrate and magnesium nitrate precursor solution mix, and are then added drop-wise in ammonium phosphate salt precursor solution by this mixed solution,
Wherein the mol ratio of (calcium+magnesium)/phosphorus is 1.67, is stirred continuously simultaneously, and in reaction, constantly dropping ammonia makes the pH value of mixed solution
Constant 10;After precursor solution drips, continue stirring 1h, to ensure fully reaction, obtain white mixed solution.Then
Being aged 20 hours by mixed solution, mixture is divided into two-layer, and upper strata is settled solution, and lower floor is white precipitate.
3, eccentric cleaning technique: mixture is centrifuged, and with distilled water, the precipitate obtained is carried out, repeat
Eccentric cleaning 3 times, then uses ethanol purge 1 time.The terpineol ethanol solution of configuration 5%, and by solid-to-liquid ratio about 1g/ml
After the white depositions that obtains adds appropriate terpineol ethanol solution, stir.
4, Technology for Heating Processing: the white mixture obtained is put into baking oven, dries 20h, obtains white powder for 80 DEG C, then at
600 DEG C of calcinings, are incubated 3h, obtain heavy metals ionic adsorption magnesium-hydroxyapatite adsorbent.
Embodiment 2
1, the preparation of precursor solution: the calcium nitrate (Ca (NO of the 0.3mol/L being respectively configured3)2) aqueous solution, 0.3mol/L
Magnesium nitrate (Mg (NO3)2) aqueous solution, the ammonium phosphate of 0.18mol/L and ammonium hydrogen phosphate ((NH4)3PO4+(NH4)2HPO4) water-soluble
Liquid, is each uniformly mixing to obtain three kinds of precursor solution;
2, chemical precipitation technique: under normal temperature condition, is 12% general by the molfraction of magnesium ion/(calcium ion+magnesium ion)
Calcium nitrate and magnesium nitrate precursor solution mix, and are then added drop-wise in ammonium phosphate salt precursor solution by this mixed solution,
Wherein the mol ratio of (calcium+magnesium)/phosphorus is 1.67, is stirred continuously simultaneously, and in reaction, constantly dropping ammonia makes the pH value of mixed solution
Constant 10.5;After precursor solution drips, continue stirring 1.5h, to ensure fully reaction, obtain white mixed solution.
Then being aged 12 hours by mixed solution, mixture is divided into two-layer, and upper strata is settled solution, and lower floor is white precipitate.
3, eccentric cleaning technique: mixture is centrifuged, and with distilled water, the precipitate obtained is carried out, repeat
Eccentric cleaning 3 times, then uses ethanol purge 2 times.The terpineol ethanol solution of configuration 5%, and by solid-to-liquid ratio about 1g/ml
After the white depositions that obtains adds appropriate terpineol ethanol solution, stir.
4, Technology for Heating Processing: the white mixture obtained is put into baking oven, dries 12h, obtains white powder for 80 DEG C, then at
800 DEG C of calcinings, are incubated 2h, obtain heavy metals ionic adsorption magnesium-hydroxyapatite adsorbent.
Embodiment 3
1, the preparation of precursor solution: the calcium nitrate (Ca (NO of the 0.5mol/L being respectively configured3)2) aqueous solution, 0.5mol/L
Magnesium nitrate (Mg (NO3)2) aqueous solution, the ammonium phosphate ((NH of 0.3mol/L4)3PO4) aqueous solution, each it is uniformly mixing to obtain three kinds
Precursor solution;
2, chemical precipitation technique: under normal temperature condition, is 10% general by the molfraction of magnesium ion/(calcium ion+magnesium ion)
Calcium nitrate and magnesium nitrate precursor solution mix, and are then added drop-wise in ammonium phosphate salt precursor solution by this mixed solution,
Wherein the mol ratio of (calcium+magnesium)/phosphorus is 1.67, is stirred continuously simultaneously, and in reaction, constantly dropping ammonia makes the pH value of mixed solution
Constant 11;After precursor solution drips, continue stirring 2h, to ensure fully reaction, obtain white mixed solution.Then
Being aged 24 hours by mixed solution, mixture is divided into two-layer, and upper strata is settled solution, and lower floor is white precipitate.
3, eccentric cleaning technique: mixture is centrifuged, and with distilled water, the precipitate obtained is carried out, repeat
Eccentric cleaning 2 times, then uses ethanol purge 2 times.The terpineol ethanol solution of configuration 5%, and by solid-to-liquid ratio about 1g/ml
After the white depositions that obtains adds appropriate terpineol ethanol solution, stir.
4, Technology for Heating Processing: the white mixture obtained is put into baking oven, dries 24h, obtains white powder for 80 DEG C, then at
700 DEG C of calcinings, are incubated 3h, obtain heavy metals ionic adsorption magnesium-hydroxyapatite adsorbent.
Embodiment 4
1, the preparation of precursor solution: the calcium nitrate (Ca (NO of the 0.75mol/L being respectively configured3)2) aqueous solution,
Magnesium nitrate (Mg (the NO of 0.75mol/L3)2) aqueous solution, the ammonium phosphate of 0.45mol/L and ammonium dihydrogen phosphate ((NH4)3PO4+(NH4)
H2PO4) aqueous solution, each it is uniformly mixing to obtain three kinds of precursor solution;
2, chemical precipitation technique: under normal temperature condition, is 7% by nitre by the molfraction of magnesium ion/(calcium ion+magnesium ion)
Acid calcium and magnesium nitrate precursor solution mix, and are then added drop-wise in ammonium phosphate salt precursor solution by this mixed solution, its
In the mol ratio of (calcium+magnesium)/phosphorus be 1.67, be stirred continuously simultaneously, in reaction, constantly dropping ammonia makes the pH value of mixed solution permanent
It is scheduled on 11.5;After precursor solution drips, continue stirring 1.5h, to ensure fully reaction, obtain white mixed solution.So
After by mixed solution be aged 8 hours, mixture is divided into two-layer, and upper strata is settled solution, and lower floor is white precipitate.
3, eccentric cleaning technique: mixture is centrifuged, and with distilled water, the precipitate obtained is carried out, repeat
Eccentric cleaning 2 times, then uses ethanol purge 1 time.The terpineol ethanol solution of configuration 5%, and by solid-to-liquid ratio about 1g/ml
After the white depositions that obtains adds appropriate terpineol ethanol solution, stir.
4, Technology for Heating Processing: the white mixture obtained is put into baking oven, dries 16h, obtains white powder for 80 DEG C, then at
700 DEG C of calcinings, are incubated 4h, obtain heavy metals ionic adsorption magnesium-hydroxyapatite adsorbent.
Embodiment 5
1, the preparation of precursor solution: the calcium nitrate (Ca (NO of the 1mol/L being respectively configured3)2) aqueous solution, the nitre of 1mol/L
Acid magnesium (Mg (NO3)2) aqueous solution, the ammonium dihydrogen phosphate ((NH of 0.6mol/L4)H2PO4) aqueous solution, each it is uniformly mixing to obtain three
Plant precursor solution;
2, chemical precipitation technique: under normal temperature condition, is 5% by nitre by the molfraction of magnesium ion/(calcium ion+magnesium ion)
Acid calcium and magnesium nitrate precursor solution mix, and are then added drop-wise in ammonium phosphate salt precursor solution by this mixed solution, its
In the mol ratio of (calcium+magnesium)/phosphorus be 1.67, be stirred continuously simultaneously, in reaction, constantly dropping ammonia makes the pH value of mixed solution permanent
It is scheduled on 12;After precursor solution drips, continue stirring 1h, to ensure fully reaction, obtain white mixed solution.Then will
Mixed solution is aged 16 hours, and mixture is divided into two-layer, and upper strata is settled solution, and lower floor is white precipitate.
3, eccentric cleaning technique: mixture is centrifuged, and with distilled water, the precipitate obtained is carried out, repeat
Eccentric cleaning 2 times, then uses ethanol purge 2 times.The terpineol ethanol solution of configuration 5%, and by solid-to-liquid ratio about 1g/ml
After the white depositions that obtains adds appropriate terpineol ethanol solution, stir.
4, Technology for Heating Processing: the white mixture obtained is put into baking oven, dries 20h, obtains white powder for 80 DEG C, then at
700 DEG C of calcinings, are incubated 2h, obtain heavy metals ionic adsorption magnesium-hydroxyapatite adsorbent.
Use X ray powder diffracting technology (XRD) and transmission electron microscope (TEM) to the magnesium-hydroxy-apatite obtained by embodiment 3
Stone adsorbent has carried out the analysis of composition and pattern.
Magnesium-hydroxyapatite adsorbent obtained by wherein Fig. 1 is embodiment 3 and undoped p magnesium hydroxylapatite adsorption
The XRD figure spectrum of agent, as seen from the figure, the undoped p magnesium hydroxyapatite of preparation under magnesium-hydroxyapatite adsorbent and the same terms
Adsorbent is one_to_one corresponding basic with the standard feature peak (JCPDS#09-432) of HA in the range of 2 θ are 20 °-60 °, does not the most go out
The most obvious miscellaneous peak.Contrast finds, undoped p magnesium hydroxyapatite adsorbent diffraction maximum is very sharp-pointed, and through 10% doping
The diffraction maximum passivation of magnesium-hydroxyapatite adsorbent each position, diffracted intensity weakens, and peak width substantially increases.The doping of magnesium is described
The crystal structure making hydroxyapatite adsorbent is distorted, and degree of crystallinity declines.Its average crystal grain chi is estimated according to penetrating happy formula
Very little about 20nm.
Fig. 2 is the TEM photo that embodiment 3 obtains magnesium-hydroxyapatite adsorbent, it can be seen that the distribution of particles of sample
Uniformly, and for being about 30nm, the bar-shaped crystalline substance of diameter about 10nm, further illustrating obtained magnesium-hydroxyapatite adsorbent is
Nano-scale particle.
The present invention uses visible-ultraviolet spectrophotometer to analyze the magnesium-hydroxy-apatite obtained by embodiment 3 further
Stone adsorbent is to copper ion (Cu in copper sulfate solution2+) absorbability, from the figure 3, it may be seen that undoped p magnesium hydroxyapatite inhale
The attached dose of absorption affinity to copper ion was about for 73% (depending on initial concentration and the solid-to-liquid ratio of copper ion), and 10% magnesium-hydroxyl phosphorus
Lime stone adsorbent has reached more than 80% to the adsorption rate of copper ion under the same conditions, it can be seen that, the work that the present invention proposes
Process can obtain a kind of magnesium-hydroxyapatite adsorbent, and the absorbability of heavy metal ion can be greatly improved.
Embodiment described in this specification, its formula, the be named title of technique etc. can be different.Every according to the present invention
Equivalence that structure, feature and principle described in inventional idea is done or simple change, be all included in the protection model of patent of the present invention
In enclosing.Described embodiment can be made various amendments or supplements or use by those skilled in the art
Similar mode substitutes, and without departing from the structure of the present invention or surmount scope defined in present claims, belongs to this
Bright protection domain.
Claims (6)
1. the preparation method of magnesium-hydroxyapatite adsorbent, it is characterised in that with calcium nitrate, magnesium nitrate and ammonium phosphate salt
For raw material, configure precursor solution with distilled water for solvent, precursor solution is uniformly mixed to form white through chemical precipitation technique
Color precipitates, and through repeatedly centrifuge washing, 80 DEG C dried 600-800 DEG C is thermally treated resulting in magnesium-hydroxyapatite adsorbent.
2. preparation method as claimed in claim 1, it is characterised in that the preparation of described precursor solution: be respectively configured
The calcium nitrate aqueous solution of 0.1-1mol/L, the magnesium nitrate aqueous solution of 0.1-1mol/L, the ammonium phosphate salt of 0.06-0.6mol/L is water-soluble
Liquid, is each uniformly mixing to obtain three kinds of precursor solution.
3. preparation method as claimed in claim 1, it is characterised in that described chemical precipitation technique: under normal temperature condition, by magnesium from
The molfraction of son/(calcium ion+magnesium ion) is that calcium nitrate and magnesium nitrate precursor solution are mixed by 5-15%, then will
This mixed solution is added drop-wise in ammonium phosphate salt precursor solution, and wherein the mol ratio of (calcium+magnesium)/phosphorus is 1.67, constantly stirs simultaneously
Mixing, the pH value that in reaction, continuous dropping ammonia makes mixed solution is constant at 10-12;After precursor solution drips, continue to stir
Mix 1-2h, to ensure fully reaction, obtain white mixed solution;Then being aged 8-24 hour by mixed solution, mixture is divided into
Two-layer, upper strata is settled solution, and lower floor is white precipitate.
4. preparation method as claimed in claim 1, it is characterised in that described centrifuge washing technique: mixture is centrifuged,
And with distilled water, the precipitate obtained is carried out, repeated centrifugation is cleaned 2-3 time, then uses ethanol purge 1-2 time;Configuration
The terpineol ethanol solution of 5%, and in the white depositions finally obtained, add appropriate terpineol by solid-to-liquid ratio about 1g/ml
Ethanol solution, stirs.
5. preparation method as claimed in claim 1, it is characterised in that described Technology for Heating Processing: the white mixture that will obtain
Put into baking oven, dry 12-24h, obtain white powder for 80 DEG C, then at 600-800 DEG C of calcining, be incubated 2-4h, obtain a waste water huge sum of money
Belong to ionic adsorption magnesium-hydroxyapatite adsorbent.
6. the preparation method as described in Claims 1 to 5 is arbitrary, it is characterised in that described ammonium phosphate salt is ammonium phosphate, phosphoric acid hydrogen
Ammonium, one or more mixture of ammonium dihydrogen phosphate.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108439360A (en) * | 2018-03-26 | 2018-08-24 | 广东药科大学附属第医院 | A kind of preparation method of spherical porous nanometer hydroxyapatite |
CN110252261A (en) * | 2019-06-21 | 2019-09-20 | 南京信息工程大学 | A kind of resin-base nano hydroxyapatite composite material, preparation method and the application in the processing of fluoride pollution water body |
CN111266080A (en) * | 2020-02-20 | 2020-06-12 | 中国科学院生态环境研究中心 | Modified HAP composite material for removing fluoride in water body, and preparation method and application thereof |
CN116371350A (en) * | 2023-03-20 | 2023-07-04 | 北京铭泽源环境工程有限公司 | Preparation method of hydroxyapatite-loaded defluorination adsorbent and defluorination adsorbent |
PL441354A1 (en) * | 2022-06-01 | 2023-12-04 | Uniwersytet Marii Curie-Skłodowskiej | Method of obtaining a sorbent of heavy metals from aqueous environments and sewage |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999032400A1 (en) * | 1997-12-22 | 1999-07-01 | Abonetics Limited | Process for the preparation of magnesium and carbonate substituted hydroxyapatite |
CN101603160A (en) * | 2009-07-07 | 2009-12-16 | 重庆大学 | Hydroxyapatite crystal whisker/magnesium metal base composite material and preparation method thereof |
CN103342555A (en) * | 2013-07-05 | 2013-10-09 | 北京北达燕园微构分析测试中心有限公司 | Strontium magnesium-doped nano-hydroxyapatite and preparation method thereof |
CN105457090A (en) * | 2014-09-04 | 2016-04-06 | 上海交通大学医学院附属瑞金医院 | Magnesium partially-substituted hydroxyapatite fiber and preparation method and application thereof |
-
2016
- 2016-10-18 CN CN201610905507.0A patent/CN106268614B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1999032400A1 (en) * | 1997-12-22 | 1999-07-01 | Abonetics Limited | Process for the preparation of magnesium and carbonate substituted hydroxyapatite |
CN101603160A (en) * | 2009-07-07 | 2009-12-16 | 重庆大学 | Hydroxyapatite crystal whisker/magnesium metal base composite material and preparation method thereof |
CN103342555A (en) * | 2013-07-05 | 2013-10-09 | 北京北达燕园微构分析测试中心有限公司 | Strontium magnesium-doped nano-hydroxyapatite and preparation method thereof |
CN105457090A (en) * | 2014-09-04 | 2016-04-06 | 上海交通大学医学院附属瑞金医院 | Magnesium partially-substituted hydroxyapatite fiber and preparation method and application thereof |
Non-Patent Citations (2)
Title |
---|
ARGHAVAN FARZADI,ET AL: "Magnesium incorporated hydroxyapatite: Synthesis and structural properties characterization", 《CERAMICS INTERNATIONAL》 * |
梁建超等: "分散剂对ZrO2料浆及陶瓷性能的影响", 《硅酸盐通报》 * |
Cited By (5)
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CN108439360A (en) * | 2018-03-26 | 2018-08-24 | 广东药科大学附属第医院 | A kind of preparation method of spherical porous nanometer hydroxyapatite |
CN110252261A (en) * | 2019-06-21 | 2019-09-20 | 南京信息工程大学 | A kind of resin-base nano hydroxyapatite composite material, preparation method and the application in the processing of fluoride pollution water body |
CN111266080A (en) * | 2020-02-20 | 2020-06-12 | 中国科学院生态环境研究中心 | Modified HAP composite material for removing fluoride in water body, and preparation method and application thereof |
PL441354A1 (en) * | 2022-06-01 | 2023-12-04 | Uniwersytet Marii Curie-Skłodowskiej | Method of obtaining a sorbent of heavy metals from aqueous environments and sewage |
CN116371350A (en) * | 2023-03-20 | 2023-07-04 | 北京铭泽源环境工程有限公司 | Preparation method of hydroxyapatite-loaded defluorination adsorbent and defluorination adsorbent |
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